Process for making insoluble bodies derived from phenol alcohols.



' a citizen of the United a 'Patent No: 350,180, 1 15,517 of 1905, and

3 LED H.

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may concern 1- Lno H. BAEKELAND, States, residing at Yonkers, in thecounty of Westchester and New York, have invented certain new and usefulImprovements in Processes for Making Insoluble Bodies Derived fromPhenol Alcohols, of which the following is a specification.

It'has been heretofore shown (see French British Patent No. GermanPatent No. 189,262, to Fabriques de Produits de Chimie OrganiquedeLaire) that phenol-alcohols, such for example as ortho-oxybenzyl alco-*Be it known that I,

hol (saligenin) and paraoxybenzyl alcohol,

yield 'by ehminationof water, resinous bodies or anhydri'ds which aresoluble" in alkaline solutions and in certain organic solvents, andwhich melt at 110 C., or above. I have also shown (see On soluble,fusible, resinous condensation products of phenols and formaldehyde, L.Backeland, J OIM'MZ of I ndustfial and Engineer-mg Chemistry, August,1909), that similar products" are obtained by heating phenol-alcohols inpresence of a very small excess of phenol, the products thus obtainedbeing characterized by great fu'si-bility and solubility.

The present invention relates to the treatment of phenol-alcohols ortheir anhydrids to produce bodies in such condition as regardshomogeneity and .texture that they can be used for various technicalpurposes.

My process, as broadly described and claimed in mycopending applicationSer. No. 520,850, filed October 4, 1909, and which has matured intoPatent #1,14:6,045, of which the present application is a division,consists in heating phenol-alcohols or their anhydrids, under pressure,for instance in a hot hydraulic press or mold, so as to obtain a hardcoherent mass or molded body of great strength and hardness, fusible,and not soluble in or greatly affected by solvents or chemicals, andwhich can be used for several of the purposes for which rubber orcelluloid have been employed heretofore.

Accordingto the invention which is the subject-matter of the presentdivisional application, the preparation of such hard, coherent massesor'inolded' articles is faciliwhich is m- 1 magnum, or ronxnns, imwYORK, nssrcnon '10 ennnnnr. BAKELITE' or new vonx, N. Y A conronn'rronor NEW YORK.-.

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Specification!!! Letters Patent. Patented J 1119 13, 1916, filed-October4, 1 09, 5am no. azcg'sso. Divided and this application Serial No.28,310

rtated bythe addition to the phenol-alcohols or their anhydrids,

before hardening them under pressure, of so-called condensing,-

agents having abasic character. As illustrative examples of suchcondensing-agents,

I may mention such basic substances as are described in my prior PatentNo. 942,809, to wit, ammonia, anhydrous or aqueous, ammonium carbonate,caustic alkalis or their carbonates anilin or pyridin, barium,strontium, or calcium, etc. Amins and amids, and in general allderivatives of the type NH, which possess basic properties, may be used,as. may also allbasicsalts,

' or salts which by secondary reaction engender bases, as for instance,alkali sulfids, acetates and cyanids, sodium triphosphate, borax, soaps,and the like.

The bases above referred to, and others the hydrates of having therequisite basic properties, are employed in variable proportionsaccording to their character and also according to the result desired.Even when used "in relatively vey small proportions they are efiectivefor the purpose described.

Instead of using phenol-alcohols, or their anyhydrids alone, it is verydesirable to mcorporate therewith suitable filling materials 1 I suchfor example other substances which tend to" improve the physical orchemical qualities of the final product. Such addition may be made atany time before the final treatment by heat and pressure. I Under thename of phenol-alcohols, I desireto designate not only the first memberof the group, oxybenzyl-alcohol, but the homologues or mixtures, ofthese products as obtained by the suitable treatment of commercialphenols or cresols. The term phenol-alcohols' is employed in the claimsto 'Lmiludethe partial anhydrids of such alcoo s. Y

When the process is app ment of phenol-alcohols, these are dehydrated bycautious heating, for example. in the manner described by De Laire, andthe as wood fiber, ground as- 'bestos, lampblack and other pigments, or

lied to the treatresulting resinous anhydrids, preferably pulinfusiblebodies or are decidedly less hard and less resistant to heat and tosolvents, than the products which are obtained by reacting upon thephenolalcohols or their anhydrids with additional quantities offormaldehyde or its equivalents, as described in my Patent N o. 1,038,475, dated September 10, 1912, and are not transformable into the latterclass of products by simple heating under any conditions- Instead ofstarting with the phenol-alcohols, I may of course prepare theiranyhydrids by direct reaction of phenols and formaldehyde, alone or inpresence of suitable condensing-agents, as for example by any of themethods described in my publication above referred to. In saidpublication, I have designated the a-nhydrids to the treatment of whichthe present invention relates under the general title of soluble,fusible resinous condensation products of phenols and formaldehyde.

The term anhydrids include both the partial and complete anhydrids ofphenol-alcohols, or in general all dehydration products thereof, knownalso collectively as saliretins/ shellac substitutes, etc. irrespectiveof the manner in which such anhydrids may have been prepared.

I claim 1. A process of making hard, compact and molded articles, whichconsists in eliminating Water from phenolis herein used to alcohols, andhardening the material by the action of heat and .a pressuresubstantially above atmospheric pressure, in presence of a basiccondensing-agent.

2. A process of making hard, compact and infusible bodies or moldedarticles, which consists in eliminating water from phenolalcohols, andhardening the composition, in

' presence of suitable filling materials and of a basiccondensing-agent, by the action of heat and a pressure substantiallyabove atmospheric pressure.

In a process of making hard, compact and infusible bodies or moldedarticles, the step which consists in hardening anhydrids ofphenol-alcohols by the action of heat and a pressure substantially aboveatmospheric pressure, and in presence of a basic condens- Ling-agent.

4. In a process of making hard, compact, and infusible bodies or moldedarticles, the step which consists in hardening anhydrids ofphenol-alcohols in presence of suitable filling materials and of a basiccondensingagent, by the action of heat and a pressure substantiallyabove atmospheric pressure.

In testimony whereof I affix my signature in presence of two witnesses.

LEO H. BAEKELAND. *lVitnesses JOHN H. THOMAS, JOHN O. lVnsToN.

